#------------------------------------------------------------------------------
#$Date: 2016-03-24 02:38:42 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179590 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/55/4505567.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4505567
loop_
_publ_author_name
'Liu, Wen-Ting'
'Li, Jin-Yan'
'Ni, Zhao-Ping'
'Bao, Xin'
'Ou, Yong-Cong'
'Leng, Ji-Dong'
'Liu, Jun-Liang'
'Tong, Ming-Liang'
_publ_section_title
;
 Incomplete Spin Crossover versus Antiferromagnetic Behavior Exhibited in
 Three-Dimensional Porous Fe(II)-Bis(tetrazolate) Frameworks
;
_journal_issue                   3
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              1482
_journal_paper_doi               10.1021/cg201569m
_journal_volume                  12
_journal_year                    2012
_chemical_formula_sum            'C46 H80 Fe3 N24 O17'
_chemical_formula_weight         1408.89
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.264(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.114(3)
_cell_length_b                   24.506(5)
_cell_length_c                   11.950(3)
_cell_measurement_temperature    298(2)
_cell_volume                     3328.0(14)
_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'PROCESS-AUTO (Rigaku, 1998)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IP'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1304
_diffrn_reflns_av_sigmaI/netI    0.1432
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10619
_diffrn_reflns_theta_full        26.99
_diffrn_reflns_theta_max         26.99
_diffrn_reflns_theta_min         3.07
_exptl_absorpt_coefficient_mu    0.725
_exptl_absorpt_correction_T_max  0.9376
_exptl_absorpt_correction_T_min  0.8866
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1476
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_platon_squeeze_details
;
;
_refine_diff_density_max         0.947
_refine_diff_density_min         -1.009
_refine_diff_density_rms         0.133
_refine_ls_extinction_coef       0.0095(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.901
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         3655
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      0.906
_refine_ls_R_factor_all          0.1407
_refine_ls_R_factor_gt           0.0914
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1669P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2305
_refine_ls_wR_factor_ref         0.2825
_reflns_number_gt                1648
_reflns_number_total             3655
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg201569m_si_001.cif
_cod_data_source_block           2.5n-BuOH(298K)
_cod_original_cell_volume        3327.9(13)
_cod_original_sg_symbol_H-M      C2/m
_cod_database_code               4505567
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Fe1 Fe 0.5000 0.5000 0.0000 0.0407(5) Uani 1 4 d S
Fe2 Fe 0.39478(10) 0.5000 0.26032(11) 0.0476(4) Uani 1 2 d S
N1 N 0.7316(5) 0.5000 0.2135(8) 0.061(2) Uani 1 2 d S
H1N H 0.7786 0.5000 0.1683 0.074 Uiso 0.17 2 d SPR
N2 N 0.6168(5) 0.5000 0.1779(6) 0.0467(15) Uani 1 2 d S
N3 N 0.5790(6) 0.5000 0.2672(6) 0.0501(16) Uani 1 2 d S
N4 N 0.6704(6) 0.5000 0.3685(7) 0.0622(19) Uani 1 2 d S
H4N H 0.6679 0.5000 0.4432 0.075 Uiso 0.17 2 d SPR
N5 N 0.3710(4) 0.39097(19) -0.0206(5) 0.0584(13) Uani 1 1 d .
H5N H 0.3830 0.3812 -0.0846 0.070 Uiso 0.17 1 calc PR
N6 N 0.3967(4) 0.43794(17) 0.0341(4) 0.0518(12) Uani 1 1 d .
N7 N 0.3680(4) 0.43710(16) 0.1324(5) 0.0532(12) Uani 1 1 d .
N8 N 0.3178(5) 0.38952(19) 0.1382(5) 0.0637(15) Uani 1 1 d .
H8N H 0.2854 0.3787 0.1927 0.076 Uiso 0.17 1 d PR
O1 O 0.4512(4) 0.44546(15) 0.4038(4) 0.0609(11) Uani 1 1 d .
O1W O 0.2240(7) 0.5000 0.2423(8) 0.086(2) Uani 1 2 d S
H1W H 0.2023 0.4751 0.2800 0.103 Uiso 1 1 d R
C1 C 0.9779(11) 0.5000 0.3813(14) 0.106(4) Uani 1 2 d SU
H1 H 0.9671 0.5000 0.3004 0.128 Uiso 1 2 calc SR
C2 C 0.8834(9) 0.5000 0.4172(9) 0.067(2) Uani 1 2 d S
C3 C 0.9035(11) 0.5000 0.5305(14) 0.102(4) Uani 1 2 d SU
H3 H 0.8398 0.5000 0.5571 0.123 Uiso 1 2 calc SR
C4 C 0.7635(6) 0.5000 0.3359(7) 0.0514(19) Uani 1 2 d S
C5 C 0.3246(8) 0.2724(3) -0.0496(9) 0.098(3) Uani 1 1 d .
H5 H 0.3745 0.2874 -0.0855 0.117 Uiso 1 1 calc R
C6 C 0.2820(6) 0.3050(2) 0.0184(7) 0.0655(18) Uani 1 1 d .
C7 C 0.2040(7) 0.2820(3) 0.0667(9) 0.093(3) Uani 1 1 d .
H7 H 0.1707 0.3035 0.1109 0.111 Uiso 1 1 calc R
C8 C 0.3222(6) 0.3615(2) 0.0434(6) 0.0602(16) Uani 1 1 d .
C9 C 0.5000 0.4687(3) 0.5000 0.0461(17) Uani 1 2 d S
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N6 Fe1 N6 87.1(2) . 2_655
N6 Fe1 N6 92.9(2) . 6_565
N6 Fe1 N6 180.0(3) 2_655 6_565
N6 Fe1 N6 180.00(16) . 5_665
N6 Fe1 N6 92.9(2) 2_655 5_665
N6 Fe1 N6 87.1(2) 6_565 5_665
N6 Fe1 N2 87.64(18) . 5_665
N6 Fe1 N2 92.36(18) 2_655 5_665
N6 Fe1 N2 87.64(18) 6_565 5_665
N6 Fe1 N2 92.36(18) 5_665 5_665
N6 Fe1 N2 92.36(18) . .
N6 Fe1 N2 87.64(18) 2_655 .
N6 Fe1 N2 92.36(18) 6_565 .
N6 Fe1 N2 87.64(18) 5_665 .
N2 Fe1 N2 180.000(1) 5_665 .
O1W Fe2 O1 96.9(2) . 6_565
O1W Fe2 O1 96.9(2) . .
O1 Fe2 O1 79.4(2) 6_565 .
O1W Fe2 N7 91.6(2) . .
O1 Fe2 N7 169.14(19) 6_565 .
O1 Fe2 N7 92.95(17) . .
O1W Fe2 N7 91.6(2) . 6_565
O1 Fe2 N7 92.95(17) 6_565 6_565
O1 Fe2 N7 169.14(19) . 6_565
N7 Fe2 N7 93.6(3) . 6_565
O1W Fe2 N3 176.2(3) . .
O1 Fe2 N3 86.01(18) 6_565 .
O1 Fe2 N3 86.01(18) . .
N7 Fe2 N3 85.82(18) . .
N7 Fe2 N3 85.82(18) 6_565 .
N2 N1 C4 102.7(7) . .
N2 N1 H1N 128.4 . .
C4 N1 H1N 128.8 . .
N3 N2 N1 111.8(7) . .
N3 N2 Fe1 121.6(5) . .
N1 N2 Fe1 126.6(6) . .
N2 N3 N4 109.2(7) . .
N2 N3 Fe2 127.6(5) . .
N4 N3 Fe2 123.3(5) . .
C4 N4 N3 105.1(7) . .
C4 N4 H4N 128.2 . .
N3 N4 H4N 126.7 . .
N6 N5 C8 105.5(5) . .
N6 N5 H5N 127.3 . .
C8 N5 H5N 127.3 . .
N5 N6 N7 109.7(4) . .
N5 N6 Fe1 126.6(4) . .
N7 N6 Fe1 122.5(3) . .
N8 N7 N6 108.8(4) . .
N8 N7 Fe2 124.1(4) . .
N6 N7 Fe2 127.1(3) . .
N7 N8 C8 104.7(5) . .
N7 N8 H8N 127.8 . .
C8 N8 H8N 127.5 . .
C9 O1 Fe2 112.6(4) . .
Fe2 O1W H1W 116.0 . .
C2 C1 C3 120.1(12) . 5_766
C2 C1 H1 120.0 . .
C3 C1 H1 120.0 5_766 .
C3 C2 C1 117.3(12) . .
C3 C2 C4 119.1(9) . .
C1 C2 C4 123.5(11) . .
C2 C3 C1 122.6(11) . 5_766
C2 C3 H3 118.7 . .
C1 C3 H3 118.7 5_766 .
N4 C4 N1 111.2(7) . .
N4 C4 C2 124.6(8) . .
N1 C4 C2 124.2(7) . .
C6 C5 C7 122.0(7) . 7
C6 C5 H5 119.0 . .
C7 C5 H5 119.0 7 .
C5 C6 C7 117.6(5) . .
C5 C6 C8 120.6(6) . .
C7 C6 C8 121.8(6) . .
C5 C7 C6 120.4(6) 7 .
C5 C7 H7 119.8 7 .
C6 C7 H7 119.8 . .
N5 C8 N8 111.3(5) . .
N5 C8 C6 125.4(6) . .
N8 C8 C6 123.3(6) . .
O1 C9 O1 125.2(7) . 2_656
O1 C9 C9 117.4(3) . 5_666
O1 C9 C9 117.4(3) 2_656 5_666
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N6 2.098(4) .
Fe1 N6 2.098(4) 2_655
Fe1 N6 2.098(4) 6_565
Fe1 N6 2.098(4) 5_665
Fe1 N2 2.107(7) 5_665
Fe1 N2 2.107(7) .
Fe2 O1W 2.005(7) .
Fe2 O1 2.093(4) 6_565
Fe2 O1 2.093(4) .
Fe2 N7 2.115(5) .
Fe2 N7 2.115(5) 6_565
Fe2 N3 2.204(6) .
N1 N2 1.307(9) .
N1 C4 1.378(11) .
N1 H1N 0.9103 .
N2 N3 1.299(9) .
N3 N4 1.328(10) .
N4 C4 1.314(10) .
N4 H4N 0.9040 .
N5 N6 1.307(6) .
N5 C8 1.331(7) .
N5 H5N 0.8600 .
N6 N7 1.336(6) .
N7 N8 1.328(6) .
N8 C8 1.342(8) .
N8 H8N 0.9077 .
O1 C9 1.234(5) .
O1W H1W 0.8523 .
C1 C2 1.354(14) .
C1 C3 1.458(18) 5_766
C1 H1 0.9300 .
C2 C3 1.291(17) .
C2 C4 1.440(12) .
C3 C1 1.458(18) 5_766
C3 H3 0.9300 .
C5 C6 1.362(9) .
C5 C7 1.375(8) 7
C5 H5 0.9300 .
C6 C7 1.387(9) .
C6 C8 1.462(8) .
C7 C5 1.375(8) 7
C7 H7 0.9300 .
C9 O1 1.234(5) 2_656
C9 C9 1.536(14) 5_666
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
C4 N1 N2 N3 0.0 . .
C4 N1 N2 Fe1 180.000(1) . .
N6 Fe1 N2 N3 -46.52(12) . .
N6 Fe1 N2 N3 -133.48(12) 2_655 .
N6 Fe1 N2 N3 46.52(12) 6_565 .
N6 Fe1 N2 N3 133.48(12) 5_665 .
N2 Fe1 N2 N3 0(100) 5_665 .
N6 Fe1 N2 N1 133.48(12) . .
N6 Fe1 N2 N1 46.52(12) 2_655 .
N6 Fe1 N2 N1 -133.48(12) 6_565 .
N6 Fe1 N2 N1 -46.52(12) 5_665 .
N2 Fe1 N2 N1 180.0(2) 5_665 .
N1 N2 N3 N4 0.000(1) . .
Fe1 N2 N3 N4 180.000(1) . .
N1 N2 N3 Fe2 180.0 . .
Fe1 N2 N3 Fe2 0.0 . .
O1W Fe2 N3 N2 0.000(4) . .
O1 Fe2 N3 N2 -140.21(11) 6_565 .
O1 Fe2 N3 N2 140.21(11) . .
N7 Fe2 N3 N2 46.95(14) . .
N7 Fe2 N3 N2 -46.95(14) 6_565 .
O1W Fe2 N3 N4 180.000(6) . .
O1 Fe2 N3 N4 39.79(11) 6_565 .
O1 Fe2 N3 N4 -39.79(11) . .
N7 Fe2 N3 N4 -133.05(14) . .
N7 Fe2 N3 N4 133.05(14) 6_565 .
N2 N3 N4 C4 0.000(1) . .
Fe2 N3 N4 C4 180.000(1) . .
C8 N5 N6 N7 2.0(6) . .
C8 N5 N6 Fe1 169.3(4) . .
N6 Fe1 N6 N5 -35.8(4) 2_655 .
N6 Fe1 N6 N5 144.2(4) 6_565 .
N6 Fe1 N6 N5 -68(49) 5_665 .
N2 Fe1 N6 N5 56.7(5) 5_665 .
N2 Fe1 N6 N5 -123.3(5) . .
N6 Fe1 N6 N7 130.0(5) 2_655 .
N6 Fe1 N6 N7 -50.0(5) 6_565 .
N6 Fe1 N6 N7 97(48) 5_665 .
N2 Fe1 N6 N7 -137.5(4) 5_665 .
N2 Fe1 N6 N7 42.5(4) . .
N5 N6 N7 N8 -2.9(7) . .
Fe1 N6 N7 N8 -170.9(4) . .
N5 N6 N7 Fe2 177.5(4) . .
Fe1 N6 N7 Fe2 9.5(6) . .
O1W Fe2 N7 N8 -54.2(5) . .
O1 Fe2 N7 N8 87.3(10) 6_565 .
O1 Fe2 N7 N8 42.8(5) . .
N7 Fe2 N7 N8 -145.9(4) 6_565 .
N3 Fe2 N7 N8 128.6(5) . .
O1W Fe2 N7 N6 125.4(5) . .
O1 Fe2 N7 N6 -93.1(10) 6_565 .
O1 Fe2 N7 N6 -137.6(5) . .
N7 Fe2 N7 N6 33.7(6) 6_565 .
N3 Fe2 N7 N6 -51.9(5) . .
N6 N7 N8 C8 2.6(7) . .
Fe2 N7 N8 C8 -177.8(4) . .
O1W Fe2 O1 C9 -102.5(3) . .
O1 Fe2 O1 C9 -6.7(4) 6_565 .
N7 Fe2 O1 C9 165.6(3) . .
N7 Fe2 O1 C9 38.7(10) 6_565 .
N3 Fe2 O1 C9 80.0(3) . .
C3 C1 C2 C3 0.000(5) 5_766 .
C3 C1 C2 C4 180.000(3) 5_766 .
C1 C2 C3 C1 0.000(3) . 5_766
C4 C2 C3 C1 180.000(4) . 5_766
N3 N4 C4 N1 0.000(1) . .
N3 N4 C4 C2 180.000(2) . .
N2 N1 C4 N4 0.000(1) . .
N2 N1 C4 C2 180.000(2) . .
C3 C2 C4 N4 0.000(2) . .
C1 C2 C4 N4 180.000(2) . .
C3 C2 C4 N1 180.000(3) . .
C1 C2 C4 N1 0.000(2) . .
C7 C5 C6 C7 -2.6(16) 7 .
C7 C5 C6 C8 174.6(8) 7 .
C5 C6 C7 C5 2.6(16) . 7
C8 C6 C7 C5 -174.6(8) . 7
N6 N5 C8 N8 -0.3(7) . .
N6 N5 C8 C6 -178.1(6) . .
N7 N8 C8 N5 -1.4(7) . .
N7 N8 C8 C6 176.5(6) . .
C5 C6 C8 N5 21.3(12) . .
C7 C6 C8 N5 -161.7(8) . .
C5 C6 C8 N8 -156.3(8) . .
C7 C6 C8 N8 20.8(12) . .
Fe2 O1 C9 O1 -174.2(3) . 2_656
Fe2 O1 C9 C9 5.8(3) . 5_666
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.020 0.464 -0.031 1866 361 ' '
